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Triethylamine → HCID 54552546, 화합물

HRID 362900
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HRID 362900 반응식
O=S(Cl)Cl.[CH3:5][O:6][C:7]1[C:8]([N+:18]([O-:20])=[O:19])=[C:9]([CH:13]=[C:14]([O:16][CH3:17])[CH:15]=1)[C:10]([OH:12])=O.[NH2:21][CH:22]1[CH2:27][CH2:26][N:25]([CH:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH2:24][CH2:23]1.C(N(CC)CC)C>C(Cl)(Cl)Cl.C1COCC1.CN(C=O)C>[CH3:5][O:6][C:7]1[C:8]([N+:18]([O-:20])=[O:19])=[C:9]([CH:13]=[C:14]([O:16][CH3:17])[CH:15]=1)[C:10]([NH:21][CH:22]1[CH2:27][CH2:26][N:25]([CH:28]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH2:24][CH2:23]1)=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 7472021HCID 7472021, 화합물HCID 128755351-(Diphenylmethyl)-4-piperidinamine

생성물 1

HCID 54552546HCID 54552546, 화합물수율 81%

시약·촉매·용매 3

HCID 6212Chloroform용매
2회
HCID 6228Dimethylformamide용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

Step 1): A solution of SOCl2 (0.5 ml, 6.6 mmol) in chloroform (10 ml) was added dropwise to a solution of 3,5-dimethoxy-2-nitrobenzoic acid [Bull. Soc. Chim. Fr., 127, 258 (1990)] (1.0 g, 4.4 mmol) and a catalytic amount of DMF in chloroform (20 ml) at room temperature. The reaction mixture was refluxed for 1 hour and then concentrated. The residue was dissolved in THF (10 ml). The THF solution was added dropwise to a solution of 4-amino-1-diphenylmethylpiperidine (1.2 g, 4.4 mmol) and triethylamine (0.5 ml, 6.6 mmol) in THF (20 ml) at 5° C. The mixture was stirred at room temperature for 1 hour and then concentrated. The residue was dissolved in ethyl acetate and washed with water. The organic layer was dried (MgSO4) and concentrated. The residue was purified by column chromatography on silica gel (10% ethyl acetate in dichloromethane) to give 3,5-dimethoxy-2-nitro-N-(1-diphenylmethylpiperidin-4-yl)benzamide (81.0%): mp 148°-150° C.

후처리

  1. customat room temperature
  2. temperatureThe reaction mixture was refluxed for 1 hour
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in THF (10 ml)
  5. concentrationconcentrated
  6. dissolutionThe residue was dissolved in ethyl acetate
  7. washwashed with water
  8. dry with materialThe organic layer was dried (MgSO4)
  9. concentrationconcentrated
  10. customThe residue was purified by column chromatography on silica gel (10% ethyl acetate in dichloromethane)

출처 및 근거

ORD 기록
ord-d60adb7ba0df4aa2bbd7511c9155db18
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05872115

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